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Ammonium Acetate → HCID 54187452、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Acetate | HCID 517165 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | (2R,5S)-5-Chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzaldehyde | HCID 53673807 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 54187452 | HCID 54187452 | 99.1% |
反応手順
To a solution of (2R,5S)-5-chloro-2-{2-[4-(4-fluoro-benzyl)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-benzaldehyde (1.86 g, 4.44 mmol) in MeOH (20 mL) was added ammonium acetate (3.42 g, 44 mmol) and sodium cyanoborohydride (0.195 g, 3.1 mmol). The resulting mixture was stirred overnight at ambient temperature. The reaction was quenched with concentrated hydrochloric acid and concentrated in vacuo. The residue was dissolved in water and basified with aqueous 3N NaOH (pH>10). The product was extracted with dichloromethane (2×) and ethyl acetate (2×). The combined organics were dried over magnesium sulfate, filtered and concentrated in vacuo. Chromatography on silica gel gave the title compound (1.29 g, 69% yield)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06649611B2 |
| 出典データセット | uspto-grants-2003_11 |
| ORD ID | ord-c4ef7363554341ffa01d88267800552d |
| 出典メモ | uspto-grants-2003_11 |